反应详情

To methyl 4-amino-6-bromo-3-methoxypyridine-2-carboxylate (0.300 g, 1.15 mmol) in 10 mL of methanol was added 1N NaOH (1.15 mL, 1.15 mmol). The reaction mixture was stirred at room temperature for 1 hr and concentrated to dryness in vacuo. Diethyl ether and H2O were added. The aqueous layer was acidified with 1N HCl until pH=2 and concentrated to dryness. Methanol (50 mL) was added to the white solid. The mixture was filtered and the filtrate concentrated to dryness. Triturating with 5% diethyl ether/pet ether gave 0.180 g of a light pink solid. 1H NMR(DMSO): δ 3.60 (s, 3H); 6.80 (S, 1H).

1. concentrationconcentrated to dryness in vacuo
2. additionDiethyl ether and H2O were added
3. concentrationconcentrated to dryness
4. additionMethanol (50 mL) was added to the white solid
5. filtrationThe mixture was filtered
6. concentrationthe filtrate concentrated to dryness
7. customTriturating with 5% diethyl ether/pet ether